JP2008157895A - Sample introducing device - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a sample introducing device for introducing a sample capable of carrying out elementary analysis with high sensitivity, by an element analyzer such as an ICP mass spectrometer and an ICP emission spectrophotometer. <P>SOLUTION: An infrared irradiation device 5 for emitting an infrared ray to an atomizing port of a nebulizer 2 to heat the sample is provided in this sample introducing device of the present invention constituted to atomize the sample fog-likely into a cyclone chamber 1 by the nebulizer 2, and to introduce the sample from a feed port 11 of the cyclone chamber 1 into a plasm torch or the like of the element analyzer. A gas supply pipe 41 for supplying a carrier gas to the nebulizer 2 is heated by a heating part 42, and a cooling part 46 cools a feed pipe 12 and an introducing pipe 46 communicated with the feed port 11 of the cyclone chamber 1. A particle size of the sample atomized by the nebulizer 2 is reduced by this manner, and only the sample of reduced particle size is introduced into the plasma torch. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention relates to a sample introduction apparatus that introduces a sample to be analyzed into an elemental analysis apparatus that performs elemental analysis by measuring light emission intensity or mass of the sample.

  Conventionally, an ICP mass spectrometer (ICP-MS: ICP-Mass Spectrometer) or an ICP-optical emission spectrometer (ICP-OES; ICP-Optical Emission Spectrometer) that performs elemental analysis using an inductively coupled plasma (ICP) Elemental analyzers such as) are known. The ICP is a plasma formed by winding a dielectric coil around a quartz tube called a plasma torch to flow a high frequency current to generate an induction electric field and introducing an argon gas into the plasma torch. ICP-MS is an apparatus that performs elemental analysis by spraying a sample into a plasma at a high temperature of about 8,000 to 10,000 degrees and detecting elements ionized by the thermal energy of the plasma. ICP-OES is a device that performs elemental analysis by spectroscopically analyzing light emitted from an element by the thermal energy of plasma using a prism or the like and measuring the wavelength, intensity, and the like of the light. These elemental analyzers are characterized by being capable of analyzing multiple elements simultaneously and having high analysis sensitivity.

  ICP-MS and ICP-OES require a liquid sample to be atomized and introduced into the plasma. The ICP-MS and ICP-OES include a sample introduction device including a nebulizer and a chamber for introducing such a sample. Yes. The nebulizer of the sample introduction device is for spraying the sample liquid with a carrier gas such as argon gas, and sprays a mist-like sample into the chamber. The chamber is for separating particles having a small particle size from the atomized sample sprayed by the nebulizer and introducing them into the plasma. Since a sample having a large particle size is separated and discharged in a chamber, the efficiency of the sample introduction device is poor and the efficiency of elemental analysis may be deteriorated when the amount of discharged sample is large. In addition, since a sample having a smaller particle size has higher elemental analysis sensitivity, it is desirable that the sample sprayed from the nebulizer be as small as possible in particle size. In recent years, in order to reduce the size of sample particles, an ultrasonic nebulizer that sprays a sample using ultrasonic waves has been put to practical use.

In Patent Document 1, a liquid sample is sprayed with a nebulizer, the sprayed sample is continuously flowed through a heating chamber, a condenser and an ICP torch, and the intensity is detected by dispersing the emitted light from the sample with a monochromator. An emission spectrophotometer configured to detect the above has been proposed. The heating chamber of this emission spectrometer has both an inlet and outlet at the base and is in the form of a vertical tube sealed at the top, with the heating chamber at one focal point of the ellipsoidal reflector. A part of the sample in the heating chamber is heated by a heating bar placed at another focal point. By heating a part of the sample in the heating chamber, the particle size of the sample can be reduced, and atomic emission spectroscopic analysis can be performed efficiently.
Japanese Patent Publication No. 5-502104

  However, the emission spectrometer described in Patent Document 1 is in the form of a vertical tube in which the heating chamber has an inlet and an outlet at the base and is sealed at the top, and a part of the sample in the heating chamber is heated to the heating bar. And it is the structure heated using an ellipsoidal reflector. Therefore, depending on the path through which the sample passes from the inlet to the outlet provided at the base of the heating chamber, there is a possibility that the sample reaches the outlet without being sufficiently heated. As described above, in the configuration of the emission spectroscopic analyzer described in Patent Document 1, there is no guarantee that all of the mist-like sample sprayed by the nebulizer can be reliably heated, and there is a limit to improving the efficiency of elemental analysis. .

  This invention is made | formed in view of such a situation, The place made into the objective is set as the structure which irradiates a heating light so that the spraying opening of the nebulizer opened in the chamber may be covered. Thus, an object of the present invention is to provide a sample introduction device that can reliably heat the sample sprayed from the nebulizer and reduce the particle size of the sample.

  Another object of the present invention is to heat the sample more reliably by heating the nebulizer spray port to a higher temperature by condensing the heating beam and irradiating it to the spray port of the nebulizer. An object of the present invention is to provide a sample introduction apparatus that can perform the above-described process.

  Another object of the present invention is to cover a wide range of mist-like samples sprayed from the nebulizer by irradiating the heating light from the position facing the spray port of the nebulizer toward the spray port. Another object of the present invention is to provide a sample introduction device that can be heated by irradiation with heating light.

  Another object of the present invention is that the heating light is condensed linearly in the spray direction of the sample from the spray port of the nebulizer, so that the mist-like sample sprayed from the nebulizer An object of the present invention is to provide a sample introduction apparatus capable of heating by irradiating heating light over a wide range.

  Another object of the present invention is that the chamber has a light-transmitting property, and when the heating light is irradiated from the outside to the inside of the chamber, the portion through which the heating light is transmitted is formed in a planar shape. Therefore, an object of the present invention is to provide a sample introduction device that can easily radiate heating light from the outside to the inside of the chamber.

  Another object of the present invention is to prevent the introduction of a sample having a large particle size by cooling the sample in the delivery path connected to the delivery port of the chamber. The object is to provide a sample introduction device.

  Another object of the present invention is to spray the fuel gas in a mist by increasing the temperature of the sample by heating the carrier gas in the gas introduction path for introducing the carrier gas into the nebulizer. An object of the present invention is to provide a sample introduction apparatus capable of

  A sample introduction device according to a first aspect of the present invention is a sample introduction device comprising a chamber having a delivery port for delivering a sample and a nebulizer for spraying the sample in the chamber, wherein the nebulizer sprays the sample into the chamber. It has a spray port, and is provided with irradiation means for irradiating heating light so as to cover the spray port.

  In the present invention, the nebulizer sprays a mist-like sample in the chamber, and irradiates the sample introduction device configured to deliver the sample from the delivery port of the chamber with heating light such as infrared rays so as to cover the nebulizer spray port. Irradiation means is provided. Although the nebulizer sprays the sample, the solvent is vaporized by heating the mist-like sample by irradiation with heating light, so that the particle size of the sample can be further reduced. Further, depending on the type of sample, it is possible to vaporize a sample other than the solvent by heating. By irradiating the heating light so as to cover the spray port of the nebulizer, it is possible to irradiate all the samples sprayed from the nebulizer with the heating light, and to efficiently heat the sample. Therefore, generation of a sample with large particles that are separated and discharged in the chamber can be reduced, and the efficiency of introducing the sample into another device such as an elemental analysis device is increased.

  Further, the sample introduction apparatus according to the second invention is characterized in that the irradiation means condenses the heating light to the spray port.

  In the present invention, when the heating light beam is irradiated, the heating light beam is condensed on the spray port of the nebulizer using an optical member such as a lens or an ellipsoidal mirror. Thereby, the energy of the heating beam can be concentrated efficiently, and the sample sprayed from the nebulizer can be heated to a higher temperature.

  Moreover, the sample introduction apparatus according to the third invention is characterized in that the irradiation means irradiates the heating light from a position facing the spray port of the nebulizer toward the spray port.

  In the present invention, the irradiation means irradiates the heating light from the position facing the spray port of the nebulizer toward the spray port. Thereby, a sample is sprayed on the passage line of heating light. The nebulized sample immediately after being sprayed from the nebulizer spray port can be surely heated, and a part of the nebulized sample that has been sprayed and diffused into the chamber can be heated. Can be increased.

  Further, the sample introduction apparatus according to the fourth invention is characterized in that the irradiating means condenses the heating light linearly in the spray direction of the sample from the spray port of the nebulizer.

  In the present invention, the irradiating means condenses the heating light linearly from the spray port of the nebulizer in the spray direction of the sample. As a result, the sample is sprayed on the condensed linear heating light, and the sample passes over the condensed heating light for a long period of time, so that the particle size of the sample can be reduced more reliably. it can.

  In the sample introduction apparatus according to the fifth aspect of the invention, the irradiation means radiates heating light from the outside to the inside of the chamber, the chamber has translucency, and is heated by the irradiation means. A portion through which light is transmitted is planar.

  In the present invention, when the chamber is made of, for example, glass and has translucency, the irradiation means irradiates the vicinity of the nebulizer in the chamber with the heating light from the outside of the chamber. At this time, a part of the chamber is formed in a flat shape, the heating light is transmitted through the flat part, and the heating light is irradiated into the chamber. When the heating light is irradiated through the curved surface portion of the chamber, it becomes difficult to irradiate the heating light at a desired position because the heating light is refracted at the curved surface portion during transmission. By forming the flat portion and transmitting the heating light, it is possible to easily irradiate the desired position with the heating light.

  According to a sixth aspect of the present invention, there is provided a sample introduction apparatus comprising: a delivery path connected to the delivery port of the chamber; and a cooling means for cooling the sample in the delivery path.

  In the present invention, the sample introduction device introduces the sample delivered from the delivery port of the chamber into the other device through the delivery path, and is provided with a cooling means for cooling the sample in the delivery path. As a result, the sample having a large particle size is cooled to form water droplets, and is separated from the sample having a small particle size. Therefore, a sample having a small particle size can be more reliably introduced into another device.

  The sample introduction device according to the seventh invention comprises a gas introduction path for introducing a carrier gas for spraying into the nebulizer, and a heating means for heating the carrier gas in the gas introduction path. And

  In the present invention, it is necessary to introduce a carrier gas into the nebulizer in order to spray the sample in the form of a mist. By providing a heating wire or the like in the gas introduction passage for introducing the carrier gas, the gas introduction passage is provided. The carrier gas inside is heated. Thereby, since the temperature of the mist-like sample sprayed from a nebulizer can be raised previously, the heating of the sample by heating light can be accelerated | stimulated.

  In the case of the first aspect of the invention, heating is performed by irradiating the heating light so as to cover the spray port of the nebulizer, so that all of the mist-like sample sprayed from the nebulizer is irradiated with the heating light and heated. In addition, since the particle size of the atomized sample can be further reduced, the generation of a sample having a large particle size that is separated and discharged in the chamber can be reduced, and the sample introduction efficiency can be increased. Therefore, when this sample introduction device is used for introduction of a sample into an elemental analysis device, the efficiency of elemental analysis can be increased, and the accuracy of analysis can be improved because the particle size of the introduced sample is small. it can. In addition, sprayed samples having a large particle size contain a large amount of solvent. When such a thing is introduced into the plasma, the plasma becomes unstable, but this can be suppressed.

  Further, in the case of the second invention, the heating light beam is condensed and applied to the nebulizer spray port, thereby efficiently concentrating the energy of the heating light beam so that the nebulizer spray port having a high sample concentration is more concentrated. Since it can be heated to a high temperature, the sample sprayed from the nebulizer can be heated to a higher temperature, and the particle size of the sample can be more reliably reduced.

  Further, in the case of the third invention, the configuration is such that the heating light is irradiated from the position facing the spraying port of the nebulizer toward the spraying port, whereby the sample is sprayed on the passage line of the heating light, and the mist-like sample is formed. Since heating can be performed by irradiating heating light over a wide range, the particle size of the sample can be reduced more reliably, and the introduction efficiency of the sample can be further increased.

  Further, in the case of the fourth invention, the sample is sprayed on the collected linear heating light by condensing the heating light linearly in the spraying direction of the sample from the spray port of the nebulizer, Since the sample passes over the heating light over a long period of time, the particle size of the sample can be reduced more reliably, and the sample introduction efficiency can be more reliably increased.

  Further, in the case of the fifth invention, the chamber has translucency, and when the heating light is irradiated from the outside to the inside of the chamber, the portion of the chamber through which the heating light is transmitted is formed in a planar shape. Thus, it is possible to easily irradiate the desired position with heating light, so that the operability of the sample introduction apparatus can be improved.

  According to the sixth aspect of the invention, by introducing a configuration in which the sample in the delivery path connected to the delivery port of the chamber is cooled, introduction of a mist-like sample having a large particle size is prevented. Since a sample with a small particle size can be introduced more reliably, the efficiency of elemental analysis when the sample is introduced into the elemental analyzer can be further increased.

  Further, in the case of the seventh invention, the temperature of the mist-like sample sprayed from the nebulizer can be increased in advance by adopting a configuration in which the carrier gas in the gas introduction path for introducing the carrier gas into the nebulizer is heated. In addition, since the sample can be heated more reliably by the heating light, the particle size of the sample can be reduced more reliably and the introduction efficiency of the sample can be further increased.

  Hereinafter, the present invention will be specifically described with reference to the drawings showing embodiments thereof. FIG. 1 is a schematic diagram showing a configuration of a sample introduction apparatus according to the present invention. In the figure, reference numeral 1 denotes a cyclone chamber, and the cyclone chamber 1 is a glass hollow container having a substantially cylindrical shape. A cylindrical fixed cylinder 10 is connected to one portion of the circumferential surface of the cyclone chamber 1 so as to protrude in the tangential direction. Further, the cyclone chamber 1 has a top surface and a bottom surface that are curved in an arch shape toward the outside, and a substantially circular delivery port 11 is opened at a substantially center of the top surface. A tube 12 is continuously provided, and a sample is introduced into the plasma torch via the delivery tube 12. In the case of ICP-MS, the sample is then introduced into the mass spectrometer. In the case of ICP-OES, the light emitted from the sample is guided to the spectroscopic device by the plasma torch. Further, a drain reservoir 13 having a bottomed cylindrical shape is connected to the substantially center of the bottom surface, and the drain reservoir 13 is connected to a waste liquid tank via a drain pipe 31 connected to a discharge port 14 opened at the bottom. 33.

  The sample introduction device also includes a nebulizer 2 that sprays the sample into the cyclone chamber 1. The nebulizer 2 is a spray-type sprayer having a double tube structure of an inner tube and an outer tube made of quartz, and the axis of the fixed cylinder 10 of the cyclone chamber 1 with the tip portion where the sample spray port is opened facing inward. It is supported and fixed on the heart. Outside the cyclone chamber 1, the inner tube of the nebulizer 2 is connected to a sample tank 37 that stores the sample solution 100 via a liquid supply tube 35, and the outer tube of the nebulizer 2 is connected to a carrier gas such as argon gas. A supply source (not shown) is connected via an air supply pipe 41. The sample liquid 100 stored in the sample tank 37 is supplied to the inner pipe of the nebulizer 2 by the operation of the liquid supply pump 36 interposed in the middle of the liquid supply pipe 35. 100 is sprayed into the inside of the cyclone chamber 1 from the spray port at the tip of the inner tube by the action of a negative pressure generated in response to the injection of the carrier gas from the gas discharge port provided at the tip of the outer tube of the nebulizer 2. It is like that.

  Further, the sample introduction apparatus includes an infrared irradiator 5 that collects and irradiates infrared rays in the cyclone chamber 1. Although not shown, the infrared irradiator 5 is an infrared lamp for generating infrared rays and an optical device such as an ellipsoidal mirror or a lens as a condensing member for collecting infrared rays generated from the infrared lamps at a predetermined position. It is the structure which has a member. The infrared irradiator 5 is disposed outside the cyclone chamber 1 and transmits infrared rays through the circumferential surface of the glass cyclone chamber 1 so as to cover the spraying portion including the spraying port and the gas discharge port of the nebulizer 2. The mist-like sample sprayed from the spraying part is irradiated with infrared rays.

  FIG. 2 is a schematic diagram for explaining the arrangement of the nebulizer 2 and the infrared irradiator 5, and the nebulizer 2 and the infrared irradiator 5 are illustrated together with the planar cross section of the cyclone chamber 1. The nebulizer 2 is fixed to a fixed cylinder 10 provided so as to protrude in a tangential direction from the peripheral surface of the cyclone chamber 1, and a mist-like sample is sprayed into the cyclone chamber 1. The infrared irradiator 5 is disposed outside the cyclone chamber 1 so as to face the spray port of the nebulizer 2 in the spray direction of the nebulizer 2. A flat surface 15 is formed by projecting a part of the surface of the cyclone chamber 1 to the outside. The infrared irradiator 5 irradiates the plane 15 with infrared rays substantially perpendicularly, and from the outside of the cyclone chamber 1. Infrared rays that are traveling so as to gather in one place that is transmitted through the plane 15 to the spray port of the nebulizer 2 are irradiated.

  3 and 4 are schematic diagrams for explaining the infrared irradiation position on the nebulizer 2, in which FIG. 3 shows a schematic perspective view, and FIG. 4 shows a schematic side sectional view. Moreover, in FIG.3 and FIG.4, infrared rays are shown with the broken line. The nebulizer 2 has an inner tube 21 that tapers toward one tip, and an outer tube 22 that is larger in diameter than the inner tube 21 and tapers toward one tip, and is arranged 2 coaxially. A spray tube 23 of the nebulizer 2 is configured by a spray port 23 a provided at the tapered tip of the inner tube 21 and a gas discharge port 23 b provided at the tapered tip of the outer tube 22. ing.

  The infrared irradiator 5 condenses the infrared rays emitted from the light source by using an optical member on a lens or an ellipsoidal mirror so as to gradually narrow toward the emission destination. It passes through a flat surface 15 (not shown in FIGS. 3 and 4) formed on the surface, covers the entire spray portion 23 having a substantially circular shape of the nebulizer 2, and collects infrared rays. . The unit in the spray unit 23 is more than the energy per unit area of the heating light in the place where the heating light is finally refracted or reflected before reaching the spray unit 23 (in this embodiment, the plane 15 of the chamber 1). The light is concentrated so that the energy per area increases. That is, a region (hereinafter referred to as an infrared irradiation region) irradiated with infrared rays that are heating light from the infrared irradiator 5 through which the infrared rays pass and reach the spray unit 23 is hatched in FIG. Although shown, the side where the sample of the opening of the spraying part 23 of the nebulizer 2 is sprayed is covered with the infrared irradiation region, and all the samples sprayed from the spraying port 23a of the nebulizer 2 pass through the infrared irradiation region. It becomes. Therefore, all the mist-like samples sprayed from the spray port 23a can be heated with infrared rays. Since the sample liquid is discharged from the inner tube 21, infrared rays do not cover both the spray port 23a of the inner tube 21 and the gas discharge port 23b of the outer tube 22 constituting the spray unit 23, but instead of the inner tube 21. Although the structure which an infrared ray covers only the spraying port 23a may be sufficient, the structure which an infrared ray covers both the spraying port 23a and the gas discharge port 23b is preferable. When the infrared irradiator 5 condenses infrared rays on the spraying part 23 of the nebulizer 2, the vicinity of the spraying part 23 is heated to about 1000 ° C. to several hundreds of degrees C. Thereby, the solvent in the mist-like sample sprayed from the nebulizer 2 is vaporized, and the particle size of the sample can be further reduced.

  FIG. 5 is a schematic diagram showing another example of an infrared irradiation method for the nebulizer 2. For example, an obstacle 30 exists between the infrared irradiation device 5 (not shown in FIG. 5) and the nebulizer 2, and a part of the infrared irradiation region from the infrared irradiation device 5 to the spray unit 23 of the nebulizer 2 is The structure interrupted by the obstacle 30 may be sufficient. However, even if the sample sprayed from the nebulizer 2 passes through the region where the infrared ray is blocked in the middle, the infrared ray is sent from the infrared irradiation device 5 to the spraying portion 23 of the nebulizer 2 at least once through the infrared irradiation region. Condensing.

  Further, since the infrared irradiator 5 collects infrared rays from a position opposed to the nebulizer 2 in the spraying direction, a part of the mist-like sample sprayed from the nebulizer 2 passes through the infrared irradiation region for a long time. Heating by the infrared irradiator 5 has the highest temperature in the vicinity of the spraying part 23, which is the infrared condensing point, but the temperature rises sufficiently even on the infrared path, so that the sprayed sample By irradiating infrared rays over a long period of time, the particle size of more samples can be reduced.

  In addition, as shown in FIG. 1, the supply gas 41 connected to the outer tube 22 of the nebulizer 2 and supplying the carrier gas is wound with a heating wire 43 in the middle portion so that the carrier gas in the supply tube 41 is supplied. A heating unit 42 for heating is provided. In the heating unit 42, the carrier gas in the air supply pipe 41 is heated by raising the temperature of the heating wire 43 to about several hundred degrees C. within the heat resistance range of the air supply pipe 41. By heating the carrier gas supplied to the nebulizer 2 in advance, the temperature of the mist-like sample sprayed from the nebulizer 2 can be increased, so that the heating of the sample performed by the infrared irradiator 5 described above is promoted. It is possible to reduce the particle size of the sample more efficiently.

  Although the particle size of the sample can be reduced with high efficiency by the infrared irradiator 5 and the heating unit 42, the sample whose particle size cannot be sufficiently reduced should be an analysis target such as ICP-MS or ICP-OES. It is preferable to remove without removing. The cyclone chamber 1 can remove and discharge a sample having a relatively large particle size by the cyclone effect. In addition, the sample introduction device according to the present embodiment cools the delivery pipe 12 of the cyclone chamber 1 and the introduction pipe 45 connected to the delivery pipe 12 to introduce the sample into a plasma torch or the like. A cooling unit 46 for cooling the sample in the delivery pipe 12 and the introduction pipe 45 is provided so that a sample having a large particle size can be coagulated and separated from a sample having a small particle size.

  In the sample introduction device having the above configuration, the sample liquid 100 stored in the sample tank 37 is supplied to the inner pipe 21 of the nebulizer 2 by the operation of the liquid supply pump 36 and heated by the air supply pipe 41 by the action of the heating unit 42. By supplying the generated carrier gas to the outer tube 22 of the nebulizer 2, a high-temperature mist is generated from the spray unit 23 by the action of negative pressure generated in response to the injection of the carrier gas from the tip of the outer tube 22 of the nebulizer 2. A sample is sprayed into the cyclone chamber 1. Infrared light from the infrared irradiator 5 is collected on the spraying portion 23 of the nebulizer 2, and the sprayed sample is heated to about 1000 ° C. to several hundreds of hundred ° C., and the solvent in the sample is vaporized, thereby the sample. The particle size of becomes smaller.

  The sample sprayed from the nebulizer 2 rises toward the top surface by a cyclone air flow generated inside the cyclone chamber 1 and is sent to the delivery pipe 12 and the introduction pipe 45 from the delivery port 11 that opens at the center of the top face. . In the cyclone chamber 1, a sample having a large particle size adheres to the inner surface of the cyclone chamber 1 by the action of the cyclone air current, flows down along the bottom surface of the cyclone chamber 1, and stays in the drain pool 13 at the center of the bottom surface.

  Further, the sample in the delivery pipe 12 and the introduction pipe 45 delivered from the delivery port 11 is cooled by the cooling unit 46, and the mist-like sample having a large particle size is coagulated to be separated from the sample having a small particle size. Is done. The agglomerated sample adheres to the inner surface of the delivery pipe 12 or the introduction pipe 45 and flows down, and stays in the drain reservoir 13 provided at the lower part of the cyclone chamber 1. A sample having a small particle size is introduced into, for example, a plasma torch such as ICP-MS or ICP-OES through the introduction tube 45, and elemental analysis is performed.

  As described above, in the sample introduction device of the present embodiment, the infrared irradiator 5 collects the infrared rays so as to cover the spray unit 23 of the nebulizer 2 and heats it, thereby spraying from the spray unit 23. The sample to be processed can be reliably heated, and the particle size can be reduced efficiently. Moreover, the heating part 42 is provided in the air supply pipe 41 that supplies the carrier gas to the nebulizer 2 and the carrier gas heated in advance is supplied to the nebulizer 2, thereby increasing the temperature of the mist-like sample sprayed by the nebulizer 2. Therefore, the efficiency of heating with infrared rays can be increased. In addition, by arranging the infrared irradiator 5 at a position facing the nebulizer 2 and collecting infrared light from the facing position to the spraying portion 23 of the nebulizer 2, a wide range of mist-like samples sprayed from the nebulizer 2 can be obtained. Since it can irradiate infrared rays over the range, the efficiency of heating the sample can be further increased. Further, a configuration for forming a heating beam having a plane 15 on the peripheral surface of the cyclone chamber 1 is formed, and the infrared irradiator 5 condenses the infrared rays on the spray unit 23 of the nebulizer 2 through the plane 15. By adjusting the irradiation position by the infrared irradiator 5, the infrared irradiator 5 is less likely to be refracted when infrared rays are transmitted through the circumferential surface of the cyclone chamber 1 compared to the case where the curved surface portion of the circumferential surface of the cyclone chamber 1 is transmitted. It is easy to do. In addition, by providing a cooling unit 46 for cooling the sample in the delivery tube 12 and the introduction tube 45 of the cyclone chamber 1, a sample having a large particle size is separated and only a sample having a small particle size is introduced into a plasma torch or the like. Therefore, the accuracy of elemental analysis by ICP-MS or ICP-OES can be increased.

  In the present embodiment, the sample introduction apparatus is configured to include the cyclone chamber 1 as a chamber. However, the present invention is not limited to this, and may be configured to include a chamber having another shape, such as a spray chamber. In addition, the heating unit 42 for heating the carrier gas in the air supply pipe 41 is provided. However, the present invention is not limited to this, and a configuration in which the carrier gas at normal temperature is supplied to the nebulizer 2 without providing the heating unit 42 may be used. . Further, the cooling unit 46 for cooling the sample in the delivery tube 12 and the introduction tube 45 is provided. However, the configuration is not limited to this, and the sample heated by the infrared irradiator 5 without the cooling unit 46 being directly provided. In addition, it may be configured to be introduced into a plasma torch or the like. The heating unit 42 and the cooling unit 46 are for supplementarily increasing the action and efficiency of heating of the sample by the infrared irradiator 5, so the sample is sufficiently heated only by the infrared irradiator 5 to reduce the particle size. It is not necessary if it can be made smaller. Further, the plane 15 is formed on the peripheral surface of the cyclone chamber 1 and the infrared irradiator 5 transmits the plane 15 and collects infrared rays. However, the present invention is not limited to this, and the plane 15 is formed on the cyclone chamber 1. It is good also as a structure which the infrared rays irradiator 5 permeate | transmits the curved surface part of the cyclone chamber 1, and condenses infrared rays, without forming. In addition, the infrared irradiator 5 is disposed at the opposite position in the spray direction of the nebulizer 2, and the infrared light is condensed from the opposite position to the spray portion 23 of the nebulizer 2, but the present invention is not limited to this. It is good also as a structure which arrange | positions 5 in another position and condenses infrared rays from another position. Further, the infrared irradiator 5 may be arranged in the cyclone chamber 1. In addition, the infrared irradiator 5 has an optical member such as an infrared lamp and an ellipsoidal mirror or a lens. However, the present invention is not limited to this, and the infrared irradiator has only the optical member and is emitted from other devices. It is good also as a structure which condenses. Further, the infrared irradiator 5 may be configured not to include an optical member such as an ellipsoidal mirror or a lens, and to irradiate the spray portion 23 of the nebulizer 2 without condensing the infrared rays emitted from the light source. Moreover, although it was set as the structure which uses infrared rays for a heating, it is not restricted to this, The structure using another light ray may be sufficient.

(Modification 1)
FIG. 6 is a schematic diagram for explaining the arrangement of the nebulizer 2 and the infrared irradiator 5 of the sample introduction apparatus according to the first modification of the present invention. The nebulizer 2 and the infrared irradiator 5 are shown together with the planar cross section of the cyclone chamber 1. It is shown. The nebulizer 2 is fixed to a fixed cylinder 10 provided so as to protrude in a tangential direction from the peripheral surface of the cyclone chamber 1, and a mist-like sample is sprayed into the cyclone chamber 1. The infrared irradiator 5 is disposed outside the cyclone chamber 1, and transmits infrared rays from the direction intersecting the spraying direction of the nebulizer 2 through the glass fixing tube 10 to the spraying port (or spraying portion) of the nebulizer 2. The light is condensed.

  As described above, the infrared irradiator 5 may be disposed at a position opposite to the nebulizer 2 instead of being disposed at a position facing the nebulizer 2. For example, the infrared irradiator 5 may be disposed near the nebulizer 2 as shown in the figure. By arranging, there is an advantage that it is easy to adjust the infrared irradiation position by the infrared irradiator 5. Since the peripheral surface of the cylindrical fixed cylinder 10 is a curved surface, illustration is omitted. However, by adjusting the infrared irradiation position by the infrared irradiator 5 and the like by forming a flat surface in a portion that transmits infrared rays. It can be done easily.

(Modification 2)
FIG. 7 is a schematic perspective view for explaining an infrared irradiation position with respect to the nebulizer 2 of the sample introduction device according to the second modification of the present invention. The infrared irradiator 5a of the sample introduction apparatus according to the modified example 2 includes an infrared lamp for generating infrared rays and an optical member such as a mirror or a lens that collects infrared rays generated from the infrared lamps in only one direction. It is a configuration. For this reason, the infrared irradiator 5 shown in FIGS. 3 and 4 condenses the infrared rays at one point, but the infrared irradiator 5a of the modified example 2 shown in FIG. 7 collects the infrared rays linearly so as to cover the spray nozzle. Shine.

  The infrared irradiator 5a is disposed outside the cyclone chamber 1 (not shown in FIG. 7), passes through the glass cyclone chamber 1 and passes through the spraying portion 23 of the nebulizer 2 to transfer the sample. Infrared rays are condensed linearly in the spraying direction (see hatched region A in FIG. 7). Thereby, about the area | region A of the fixed distance from the spraying part 23, the sample sprayed from the nebulizer 2 can be heated at high temperature, and a sample can be heated more efficiently and particle size can be made small.

  The infrared irradiator 5a collects and irradiates infrared rays. However, the present invention is not limited to this. For example, the infrared irradiator 5a may be configured to irradiate heating light in an appropriate mode such as parallel light or diffused light. Good.

(Modification 3)
FIG. 8 is a schematic diagram for explaining an infrared irradiation position with respect to the nebulizer 2 of the sample introduction device according to the third modification of the present invention. As shown in FIG. 8, the focal point B of infrared rays collected by the infrared irradiator (the portion where the energy per unit area of infrared rays is the largest) is aligned with the front side of the spraying portion 23 of the nebulizer 2, and the focal point B ahead of the focal point B. It is also possible to adopt a configuration in which the infrared irradiation region covers the spray portion 23. By setting it as such a structure, since the focus B of the infrared rays with the highest temperature is outside the nebulizer 2, it is possible to suppress the occurrence of damage such as melting of the nebulizer 2 due to heat.

It is a schematic diagram which shows the structure of the sample introduction apparatus which concerns on this invention. It is a schematic diagram for demonstrating arrangement | positioning of a nebulizer and an infrared irradiation device. It is a schematic diagram for demonstrating the irradiation position of the infrared rays with respect to a nebulizer. It is a schematic diagram for demonstrating the irradiation position of the infrared rays with respect to a nebulizer. It is a schematic diagram which shows the other example of the infrared irradiation method with respect to a nebulizer. It is a schematic diagram for demonstrating arrangement | positioning of the nebulizer and infrared rays irradiator of the sample introduction apparatus which concerns on the modification 1 of this invention. It is a typical perspective view for demonstrating the irradiation position of the infrared rays with respect to the nebulizer of the sample introduction apparatus which concerns on the modification 2 of this invention. It is a schematic diagram for demonstrating the irradiation position of the infrared rays with respect to the nebulizer of the sample introduction apparatus which concerns on the modification 3 of this invention.

Explanation of symbols

1 Cyclone chamber 2 Nebulizer 5 Infrared irradiator (irradiation means)
10 fixed cylinder 11 delivery port 12 delivery pipe (delivery path)
13 Drain pool 15 Plane 21 Inner cylinder 22 Outer cylinder 23 Spray part 23a Spray port 23b Gas discharge port 41 Air supply pipe (gas introduction path)
42 Heating part (heating means)
43 Heating wire 45 Introduction pipe (delivery path)
46 Cooling part (cooling means)

Claims (7)

In a sample introduction apparatus comprising a chamber having a delivery port for delivering a sample, and a nebulizer for spraying the sample in the chamber,
The nebulizer has a spray port for spraying a sample in the chamber,
A sample introduction apparatus comprising irradiation means for irradiating heating light so as to cover the spray port.   The sample introduction apparatus according to claim 1, wherein the irradiating means condenses heating light to the spray port.   3. The sample introduction device according to claim 1, wherein the irradiating unit irradiates the heating light from a position facing the spray port of the nebulizer toward the spray port. 4.   3. The sample introduction apparatus according to claim 2, wherein the irradiation means condenses the heating light in a line shape from the spray port of the nebulizer in the spray direction of the sample. The irradiation means radiates heating light from the outside to the inside of the chamber,
The sample introduction apparatus according to any one of claims 1 to 4, wherein the chamber has a light-transmitting property, and a portion through which the heating light from the irradiation unit is transmitted is planar. A delivery path connected to the delivery port of the chamber;
The sample introduction device according to claim 1, further comprising: a cooling unit that cools the sample in the delivery path. A gas introduction path for introducing a carrier gas for spraying into the nebulizer;
The sample introduction device according to claim 1, further comprising: a heating unit that heats the carrier gas in the gas introduction path.

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